Dichloromethane → HCID 178448704, 화합물

HRID 1199746노트

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HRID 1199746 반응식
[CH2:1]([N:5]1[C:12](=[O:13])[CH2:11][C:9](=[O:10])[N:8]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4].C1(C)C=CC(S([N:29]=[N+:30]=[N-])(=O)=O)=CC=1.C(N(CC)CC)C.ClCCl>C(#N)C>[CH2:1]([N:5]1[C:12](=[O:13])[C:11](=[N+:29]=[N-:30])[C:9](=[O:10])[N:8]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 13661p-Toluenesulfonyl azideHCID 14848100HCID 14848100, 화합물

생성물 1

HCID 178448704HCID 178448704, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

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온도
2 °C

실험 절차

80 mL of reagent grade acetonitrile and 6.65 gm (0.025 mole) of 1-(1-butyl)-3-cyclohexylbarbituric acid were added to a dry 250 mL 3-neck round bottom flask equipped with a thermometer, pressure equalizing dropping funnel capped by a drying tube, nitrogen inlet and magnetic stirrer. The stirred solution was cooled to 2° C. in an ice bath. Then a solution of 5.75 gm (0.029 mole) of p-toluenesulfonyl azide in 20 mL of acetonitrile was added to the reaction flask. A solution of 3.20 gm (0.0317 mole) of triethylamine in 20 mL of reagent grade dichloromethane was placed in the dropping funnel and slowly added to the reaction flask, while keeping the temperature below 3° C. The flask temperature was kept below 3° C. for 1 hour. The stirred reaction flask was allowed to warm to room temperature (20° C.) and kept at room temperature for 12 hours.

후처리

  1. customequipped with a thermometer, pressure
  2. customcapped by a drying tube, nitrogen inlet and magnetic stirrer
  3. additionslowly added to the reaction flask
  4. customthe temperature below 3° C
  5. customThe stirred reaction flask
  6. temperatureto warm to room temperature (20° C.)
  7. waitkept at room temperature for 12 hours

출처 및 근거

ORD 기록
ord-a3aaf410ba904e71b671db5787ec800e
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04902784

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